Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal ' Dalton Transactions ' _publ_contact_author_name ' Paul E. Kruger ' _publ_contact_author_address ; Department of Chemistry Trinity College Dublin Dublin 2 Ireland ; _publ_contact_author_phone ' 353 1 608 1422 ' _publ_contact_author_fax ' 353 1 671 2826 ' _publ_contact_author_email ' paul.kruger@tcd.ie ' loop_ _publ_author_name _publ_author_address ' Paul E. Kruger ' ; School of Chemistry University of Dublin Trinity College Dublin 2 Ireland ; ' Robert P. Doyle ' ; School of Chemistry University of Dublin Trinity College Dublin 2 Ireland ; ' Mark Nieuwenhuyzen' ; Chemistry Department Queen's University Belfast, BT9 5AG UK ; ' Miguel Julve ' ; Department de Quimica Inorganica Facultat de Quimica Universitat de Valencia Dr. Molinar 50, E-46100, Valencia Spain. ; ' Francesc Lloret ' ; Department de Quimica Inorganica Facultat de Quimica Universitat de Valencia Dr. Molinar 50, E-46100, Valencia Spain. ; _publ_section_title ; Synthesis, structure and magnetic properties of polynuclear copper(II) complexes incorporating p-block oxo-anions ; data_1 _database_code_depnum_ccdc_archive 'CCDC 289114' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H48 Cu3 N6 O19' _chemical_formula_weight 1011.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7390(10) _cell_length_b 13.4550(10) _cell_length_c 18.4430(10) _cell_angle_alpha 95.740(10) _cell_angle_beta 97.550(10) _cell_angle_gamma 106.710(10) _cell_volume 2037.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.34 _cell_measurement_theta_max 12.49 _exptl_crystal_description plate _exptl_crystal_colour Blue _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.72 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 1.637 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3693 _exptl_absorpt_correction_T_max 0.8667 _exptl_absorpt_process_details 'Psi Scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 7683 _diffrn_reflns_av_R_equivalents 0.0118 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7169 _reflns_number_gt 6246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+3.1492P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7169 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.61941(5) 1.00056(3) 0.95339(2) 0.01428(11) Uani 1 1 d . . . Cu2 Cu 0.43885(4) 0.81744(3) 0.74062(2) 0.01301(11) Uani 1 1 d . . . Cu3 Cu -0.10362(4) 0.54761(3) 0.53813(2) 0.01175(11) Uani 1 1 d . . . N1A N 0.7796(3) 0.9250(2) 0.93708(15) 0.0177(6) Uani 1 1 d . . . C2A C 0.7703(4) 0.8290(3) 0.95420(19) 0.0220(7) Uani 1 1 d . . . H2A H 0.6804 0.7924 0.9751 0.026 Uiso 1 1 calc R . . C3A C 0.8877(5) 0.7819(3) 0.9422(2) 0.0286(8) Uani 1 1 d . . . H3A H 0.8786 0.7137 0.9544 0.034 Uiso 1 1 calc R . . C4A C 1.0190(5) 0.8358(3) 0.9122(2) 0.0301(9) Uani 1 1 d . . . H4A H 1.1013 0.8049 0.9038 0.036 Uiso 1 1 calc R . . C5A C 1.0297(4) 0.9351(3) 0.89451(19) 0.0254(8) Uani 1 1 d . . . H5A H 1.1193 0.9733 0.8741 0.030 Uiso 1 1 calc R . . C6A C 0.9068(4) 0.9775(3) 0.90720(18) 0.0196(7) Uani 1 1 d . . . C7A C 0.9029(4) 1.0821(3) 0.88999(18) 0.0203(7) Uani 1 1 d . . . C8A C 1.0222(5) 1.1486(3) 0.8592(2) 0.0286(8) Uani 1 1 d . . . H8A H 1.1127 1.1286 0.8473 0.034 Uiso 1 1 calc R . . C9A C 1.0054(5) 1.2449(3) 0.8464(2) 0.0349(10) Uani 1 1 d . . . H9A H 1.0853 1.2921 0.8256 0.042 Uiso 1 1 calc R . . C10A C 0.8736(5) 1.2722(3) 0.8637(2) 0.0353(9) Uani 1 1 d . . . H10A H 0.8612 1.3381 0.8549 0.042 Uiso 1 1 calc R . . C11A C 0.7583(5) 1.2019(3) 0.8942(2) 0.0262(8) Uani 1 1 d . . . H11A H 0.6662 1.2201 0.9059 0.031 Uiso 1 1 calc R . . N12A N 0.7743(3) 1.1094(2) 0.90759(15) 0.0189(6) Uani 1 1 d . . . N1B N 0.5288(3) 0.7015(2) 0.76629(15) 0.0185(6) Uani 1 1 d . . . C2B C 0.4485(5) 0.6144(3) 0.79189(19) 0.0240(8) Uani 1 1 d . . . H2B H 0.3400 0.6054 0.7992 0.029 Uiso 1 1 calc R . . C3B C 0.5189(6) 0.5381(3) 0.8077(2) 0.0334(9) Uani 1 1 d . . . H3B H 0.4614 0.4788 0.8277 0.040 Uiso 1 1 calc R . . C4B C 0.6740(5) 0.5487(3) 0.7943(2) 0.0349(10) Uani 1 1 d . . . H4B H 0.7225 0.4953 0.8030 0.042 Uiso 1 1 calc R . . C5B C 0.7587(5) 0.6382(3) 0.7679(2) 0.0292(9) Uani 1 1 d . . . H5B H 0.8659 0.6474 0.7586 0.035 Uiso 1 1 calc R . . C6B C 0.6819(4) 0.7135(3) 0.75548(18) 0.0200(7) Uani 1 1 d . . . C7B C 0.7606(4) 0.8140(3) 0.73017(18) 0.0186(7) Uani 1 1 d . . . C8B C 0.9183(4) 0.8441(3) 0.71628(19) 0.0276(8) Uani 1 1 d . . . H8B H 0.9831 0.7986 0.7215 0.033 Uiso 1 1 calc R . . C9B C 0.9802(4) 0.9416(3) 0.6946(2) 0.0323(9) Uani 1 1 d . . . H9B H 1.0884 0.9639 0.6853 0.039 Uiso 1 1 calc R . . C10B C 0.8830(5) 1.0056(3) 0.6866(2) 0.0300(9) Uani 1 1 d . . . H10B H 0.9228 1.0722 0.6712 0.036 Uiso 1 1 calc R . . C11B C 0.7269(4) 0.9715(3) 0.70116(19) 0.0219(7) Uani 1 1 d . . . H11B H 0.6603 1.0159 0.6958 0.026 Uiso 1 1 calc R . . N12B N 0.6659(3) 0.8775(2) 0.72276(15) 0.0166(6) Uani 1 1 d . . . N1C N -0.1801(3) 0.6757(2) 0.53238(14) 0.0147(6) Uani 1 1 d . . . C2C C -0.1025(4) 0.7656(3) 0.50808(18) 0.0181(7) Uani 1 1 d . . . H2C H -0.0002 0.7725 0.4934 0.022 Uiso 1 1 calc R . . C3C C -0.1671(4) 0.8471(3) 0.50396(19) 0.0215(7) Uani 1 1 d . . . H3C H -0.1106 0.9086 0.4859 0.026 Uiso 1 1 calc R . . C4C C -0.3147(4) 0.8391(3) 0.52622(19) 0.0216(7) Uani 1 1 d . . . H4C H -0.3607 0.8949 0.5238 0.026 Uiso 1 1 calc R . . C5C C -0.3945(4) 0.7480(3) 0.55226(18) 0.0184(7) Uani 1 1 d . . . H5C H -0.4956 0.7407 0.5683 0.022 Uiso 1 1 calc R . . C6C C -0.3239(4) 0.6679(3) 0.55441(16) 0.0138(6) Uani 1 1 d . . . C7C C -0.3979(4) 0.5675(2) 0.58040(16) 0.0130(6) Uani 1 1 d . . . C8C C -0.5458(4) 0.5429(3) 0.60578(18) 0.0178(7) Uani 1 1 d . . . H8C H -0.6071 0.5908 0.6060 0.021 Uiso 1 1 calc R . . C9C C -0.6017(4) 0.4473(3) 0.63071(19) 0.0203(7) Uani 1 1 d . . . H9C H -0.7019 0.4289 0.6486 0.024 Uiso 1 1 calc R . . C10C C -0.5096(4) 0.3788(3) 0.62926(19) 0.0209(7) Uani 1 1 d . . . H10C H -0.5449 0.3135 0.6470 0.025 Uiso 1 1 calc R . . C11C C -0.3668(4) 0.4065(3) 0.60188(18) 0.0173(7) Uani 1 1 d . . . H11C H -0.3057 0.3585 0.5998 0.021 Uiso 1 1 calc R . . N12C N -0.3103(3) 0.4995(2) 0.57782(14) 0.0136(5) Uani 1 1 d . . . O1 O 0.4895(3) 1.09011(17) 0.98009(12) 0.0176(5) Uani 1 1 d . . . H1O H 0.4196 1.0796 0.9322 0.026 Uiso 1 1 d R . . O2 O 0.0719(3) 0.59073(16) 0.48156(12) 0.0134(4) Uani 1 1 d . . . H2O H 0.1469 0.6388 0.5132 0.020 Uiso 1 1 d R . . C1 C 0.3953(4) 0.9791(2) 0.80833(17) 0.0144(7) Uani 1 1 d . . . O11 O 0.3612(3) 1.06096(18) 0.83204(13) 0.0204(5) Uani 1 1 d . . . O12 O 0.3823(3) 0.94916(17) 0.73813(12) 0.0156(5) Uani 1 1 d . . . O13 O 0.4443(3) 0.92096(17) 0.85205(12) 0.0157(5) Uani 1 1 d . . . C2 C 0.1686(4) 0.6840(2) 0.66329(18) 0.0138(6) Uani 1 1 d . . . O21 O 0.2532(3) 0.71681(17) 0.61377(12) 0.0174(5) Uani 1 1 d . . . O22 O 0.2179(3) 0.72882(18) 0.73157(13) 0.0177(5) Uani 1 1 d . . . O23 O 0.0376(3) 0.60709(18) 0.64843(12) 0.0188(5) Uani 1 1 d . . . O1W O 0.3747(3) 1.08283(19) 0.63975(13) 0.0245(5) Uani 1 1 d . . . H1W1 H 0.3101 1.1163 0.6502 0.037 Uiso 1 1 d R . . H1W2 H 0.3688 1.0420 0.6737 0.037 Uiso 1 1 d R . . O2W O 0.9708(3) 1.3155(2) 0.64472(15) 0.0236(6) Uani 1 1 d . . . H2W1 H 0.969(5) 1.348(4) 0.607(3) 0.035 Uiso 1 1 d . . . H2W2 H 0.891(6) 1.274(4) 0.641(3) 0.035 Uiso 1 1 d . . . O3W O 0.6702(3) 1.2616(2) 1.07963(15) 0.0322(6) Uani 1 1 d . . . H3W1 H 0.6185 1.2112 1.0343 0.048 Uiso 1 1 d R . . H3W2 H 0.6408 1.2230 1.1278 0.048 Uiso 1 1 d R . . O4W O 0.0099(4) 0.4835(2) 0.75740(14) 0.0333(6) Uani 1 1 d . . . H4W1 H 0.0085 0.5258 0.7203 0.050 Uiso 1 1 d R . . H4W2 H -0.0104 0.4274 0.7300 0.050 Uiso 1 1 d R . . O5W O 1.1943(3) 1.2096(2) 0.68394(15) 0.0297(6) Uani 1 1 d . . . H5W1 H 1.2477 1.2419 0.7280 0.045 Uiso 1 1 d R . . H5W2 H 1.1236 1.2377 0.6654 0.045 Uiso 1 1 d R . . O6W O 0.6832(3) 1.1612(2) 0.60310(15) 0.0328(6) Uani 1 1 d . . . H6W1 H 0.6692 1.1396 0.5520 0.049 Uiso 1 1 d R . . H6W2 H 0.5779 1.1426 0.6115 0.049 Uiso 1 1 d R . . O7W O 0.3144(4) 0.8931(2) 0.54383(15) 0.0386(7) Uani 1 1 d . . . H7W1 H 0.3111 0.9481 0.5677 0.058 Uiso 1 1 d R . . H7W2 H 0.2750 0.8448 0.5708 0.058 Uiso 1 1 d R . . O8W O 0.4083(4) 1.2669(2) 0.81421(18) 0.0407(7) Uani 1 1 d . . . H8W1 H 0.4158 1.2933 0.8627 0.061 Uiso 1 1 d R . . H8W2 H 0.3962 1.2033 0.8090 0.061 Uiso 1 1 d R . . O9W O 1.0587(5) 0.5625(2) 0.90328(16) 0.0564(10) Uani 1 1 d . . . H9W1 H 1.0371 0.5377 0.8493 0.085 Uiso 1 1 d R . . H9W2 H 1.1415 0.6247 0.9130 0.085 Uiso 1 1 d R . . O10W O 1.2190(7) 0.4806(3) 1.0135(2) 0.0843(15) Uani 1 1 d . . . H101 H 1.1125 0.4645 1.0297 0.126 Uiso 1 1 d R . . H102 H 1.1615 0.4967 0.9721 0.126 Uiso 1 1 d R . . O11W O 0.5558(7) 0.6281(3) 1.0454(2) 0.0915(16) Uani 1 1 d . . . H111 H 0.4359 0.5811 1.0297 0.137 Uiso 1 1 d R . . H112 H 0.6147 0.5830 1.0246 0.137 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0169(2) 0.0113(2) 0.0145(2) 0.00298(15) 0.00375(15) 0.00324(16) Cu2 0.0131(2) 0.0100(2) 0.0152(2) 0.00221(15) 0.00110(15) 0.00277(15) Cu3 0.0117(2) 0.0099(2) 0.0141(2) 0.00290(14) 0.00338(15) 0.00298(15) N1A 0.0176(14) 0.0176(14) 0.0165(14) -0.0010(11) -0.0001(11) 0.0055(12) C2A 0.0264(18) 0.0160(17) 0.0232(18) 0.0017(14) 0.0023(15) 0.0069(15) C3A 0.032(2) 0.026(2) 0.028(2) -0.0011(16) -0.0035(16) 0.0132(17) C4A 0.027(2) 0.036(2) 0.029(2) -0.0050(17) -0.0034(16) 0.0177(18) C5A 0.0196(18) 0.034(2) 0.0195(18) -0.0045(15) 0.0008(14) 0.0065(16) C6A 0.0169(16) 0.0230(18) 0.0149(16) -0.0006(14) -0.0004(13) 0.0024(14) C7A 0.0190(17) 0.0237(18) 0.0143(16) 0.0010(14) 0.0005(13) 0.0021(14) C8A 0.0249(19) 0.033(2) 0.0250(19) 0.0043(16) 0.0105(16) 0.0014(17) C9A 0.035(2) 0.029(2) 0.037(2) 0.0097(18) 0.0175(19) -0.0029(18) C10A 0.040(2) 0.025(2) 0.042(2) 0.0183(18) 0.0157(19) 0.0046(18) C11A 0.029(2) 0.0215(19) 0.029(2) 0.0097(15) 0.0075(16) 0.0056(16) N12A 0.0202(14) 0.0160(14) 0.0180(14) 0.0035(11) 0.0040(11) 0.0010(12) N1B 0.0232(15) 0.0159(14) 0.0151(14) -0.0004(11) -0.0003(11) 0.0061(12) C2B 0.034(2) 0.0159(17) 0.0213(18) 0.0049(14) 0.0036(15) 0.0050(15) C3B 0.058(3) 0.0182(19) 0.024(2) 0.0055(15) 0.0016(18) 0.0132(19) C4B 0.054(3) 0.028(2) 0.028(2) 0.0029(17) -0.0062(19) 0.027(2) C5B 0.036(2) 0.028(2) 0.0257(19) -0.0028(16) -0.0052(16) 0.0197(18) C6B 0.0252(18) 0.0213(18) 0.0132(16) -0.0023(13) -0.0039(13) 0.0117(15) C7B 0.0209(17) 0.0211(18) 0.0135(16) -0.0032(13) -0.0010(13) 0.0095(14) C8B 0.0192(18) 0.045(2) 0.0185(18) -0.0031(16) -0.0013(14) 0.0151(17) C9B 0.0153(18) 0.045(2) 0.030(2) -0.0013(18) 0.0055(15) 0.0003(17) C10B 0.0234(19) 0.028(2) 0.031(2) 0.0014(16) 0.0061(16) -0.0038(16) C11B 0.0203(17) 0.0183(17) 0.0245(18) 0.0017(14) 0.0050(14) 0.0020(14) N12B 0.0171(14) 0.0156(14) 0.0156(14) -0.0011(11) 0.0010(11) 0.0042(11) N1C 0.0153(13) 0.0140(13) 0.0137(13) 0.0019(11) 0.0014(11) 0.0031(11) C2C 0.0202(17) 0.0148(16) 0.0187(17) 0.0040(13) 0.0045(13) 0.0035(14) C3C 0.0273(19) 0.0155(17) 0.0212(17) 0.0067(14) 0.0023(14) 0.0049(14) C4C 0.0307(19) 0.0171(17) 0.0197(17) 0.0029(13) 0.0005(15) 0.0129(15) C5C 0.0200(17) 0.0184(17) 0.0175(16) 0.0003(13) 0.0014(13) 0.0084(14) C6C 0.0153(16) 0.0158(16) 0.0086(14) 0.0006(12) -0.0004(12) 0.0038(13) C7C 0.0138(15) 0.0147(16) 0.0102(15) -0.0005(12) 0.0003(12) 0.0054(13) C8C 0.0156(16) 0.0207(17) 0.0160(16) 0.0005(13) 0.0007(13) 0.0055(14) C9C 0.0166(16) 0.0218(18) 0.0194(17) -0.0012(14) 0.0043(13) 0.0016(14) C10C 0.0212(17) 0.0179(17) 0.0212(18) 0.0038(14) 0.0061(14) 0.0008(14) C11C 0.0194(16) 0.0144(16) 0.0182(16) 0.0032(13) 0.0031(13) 0.0052(13) N12C 0.0141(13) 0.0125(13) 0.0141(13) 0.0029(10) 0.0029(11) 0.0030(11) O1 0.0229(12) 0.0158(12) 0.0161(11) 0.0027(9) 0.0052(9) 0.0078(10) O2 0.0151(11) 0.0092(11) 0.0161(11) 0.0044(9) 0.0047(9) 0.0024(9) C1 0.0112(15) 0.0128(16) 0.0187(17) 0.0043(13) 0.0036(12) 0.0017(12) O11 0.0278(13) 0.0156(12) 0.0221(12) 0.0042(10) 0.0067(10) 0.0116(10) O12 0.0174(11) 0.0148(11) 0.0147(11) 0.0032(9) 0.0010(9) 0.0056(9) O13 0.0241(12) 0.0099(11) 0.0134(11) 0.0039(9) -0.0002(9) 0.0064(9) C2 0.0138(16) 0.0101(15) 0.0178(16) 0.0032(12) -0.0004(13) 0.0050(13) O21 0.0171(11) 0.0125(11) 0.0218(12) 0.0027(9) 0.0068(10) 0.0016(9) O22 0.0152(11) 0.0160(12) 0.0186(12) -0.0010(9) 0.0016(9) 0.0013(9) O23 0.0173(12) 0.0186(12) 0.0145(11) 0.0042(9) -0.0020(9) -0.0023(10) O1W 0.0334(14) 0.0227(13) 0.0243(13) 0.0144(10) 0.0100(11) 0.0131(11) O2W 0.0250(14) 0.0218(14) 0.0247(14) 0.0075(11) 0.0013(11) 0.0081(11) O3W 0.0333(15) 0.0244(14) 0.0345(15) -0.0036(12) 0.0058(12) 0.0046(12) O4W 0.0566(18) 0.0196(13) 0.0211(13) 0.0051(11) 0.0062(13) 0.0071(13) O5W 0.0235(13) 0.0307(15) 0.0397(16) 0.0137(12) 0.0061(12) 0.0123(12) O6W 0.0301(14) 0.0308(15) 0.0317(15) 0.0064(12) 0.0045(12) 0.0002(12) O7W 0.061(2) 0.0226(14) 0.0297(15) 0.0059(12) 0.0174(14) 0.0048(14) O8W 0.0473(18) 0.0203(14) 0.0522(19) 0.0134(13) -0.0026(15) 0.0091(13) O9W 0.093(3) 0.0276(16) 0.0262(16) 0.0075(13) -0.0108(17) -0.0083(17) O10W 0.152(4) 0.043(2) 0.048(2) 0.0091(17) -0.022(3) 0.031(3) O11W 0.178(5) 0.055(3) 0.054(2) 0.010(2) 0.018(3) 0.055(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.949(2) . ? Cu1 O1 1.959(2) 2_677 ? Cu1 N1A 1.988(3) . ? Cu1 N12A 2.025(3) . ? Cu1 O13 2.211(2) . ? Cu1 Cu1 2.8709(8) 2_677 ? Cu2 O22 1.931(2) . ? Cu2 O12 1.975(2) . ? Cu2 N12B 2.000(3) . ? Cu2 N1B 2.008(3) . ? Cu2 O13 2.351(2) . ? Cu2 C1 2.549(3) . ? Cu3 O2 1.951(2) . ? Cu3 O2 1.965(2) 2_566 ? Cu3 N12C 1.997(3) . ? Cu3 N1C 2.027(3) . ? Cu3 O23 2.179(2) . ? Cu3 Cu3 2.9228(8) 2_566 ? N1A C2A 1.343(5) . ? N1A C6A 1.351(5) . ? C2A C3A 1.381(5) . ? C3A C4A 1.384(6) . ? C4A C5A 1.387(6) . ? C5A C6A 1.387(5) . ? C6A C7A 1.483(5) . ? C7A N12A 1.346(5) . ? C7A C8A 1.389(5) . ? C8A C9A 1.386(6) . ? C9A C10A 1.370(6) . ? C10A C11A 1.392(5) . ? C11A N12A 1.335(5) . ? N1B C6B 1.345(5) . ? N1B C2B 1.346(5) . ? C2B C3B 1.376(5) . ? C3B C4B 1.379(6) . ? C4B C5B 1.391(6) . ? C5B C6B 1.388(5) . ? C6B C7B 1.482(5) . ? C7B N12B 1.354(4) . ? C7B C8B 1.386(5) . ? C8B C9B 1.388(6) . ? C9B C10B 1.378(6) . ? C10B C11B 1.380(5) . ? C11B N12B 1.346(5) . ? N1C C6C 1.350(4) . ? N1C C2C 1.357(4) . ? C2C C3C 1.373(5) . ? C3C C4C 1.383(5) . ? C4C C5C 1.390(5) . ? C5C C6C 1.389(5) . ? C6C C7C 1.477(4) . ? C7C N12C 1.353(4) . ? C7C C8C 1.394(5) . ? C8C C9C 1.386(5) . ? C9C C10C 1.387(5) . ? C10C C11C 1.374(5) . ? C11C N12C 1.348(4) . ? O1 Cu1 1.959(2) 2_677 ? O2 Cu3 1.965(2) 2_566 ? C1 O11 1.272(4) . ? C1 O13 1.294(4) . ? C1 O12 1.297(4) . ? C2 O23 1.279(4) . ? C2 O21 1.283(4) . ? C2 O22 1.301(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 85.45(10) . 2_677 ? O1 Cu1 N1A 171.19(11) . . ? O1 Cu1 N1A 96.24(11) 2_677 . ? O1 Cu1 N12A 95.29(11) . . ? O1 Cu1 N12A 165.65(11) 2_677 . ? N1A Cu1 N12A 80.93(12) . . ? O1 Cu1 O13 92.58(9) . . ? O1 Cu1 O13 95.88(9) 2_677 . ? N1A Cu1 O13 95.83(10) . . ? N12A Cu1 O13 98.40(10) . . ? O1 Cu1 Cu1 42.85(7) . 2_677 ? O1 Cu1 Cu1 42.59(6) 2_677 2_677 ? N1A Cu1 Cu1 138.17(9) . 2_677 ? N12A Cu1 Cu1 136.35(8) . 2_677 ? O13 Cu1 Cu1 95.77(6) . 2_677 ? O22 Cu2 O12 95.03(9) . . ? O22 Cu2 N12B 162.13(10) . . ? O12 Cu2 N12B 95.48(10) . . ? O22 Cu2 N1B 92.46(11) . . ? O12 Cu2 N1B 166.31(10) . . ? N12B Cu2 N1B 80.37(11) . . ? O22 Cu2 O13 96.51(9) . . ? O12 Cu2 O13 60.31(8) . . ? N12B Cu2 O13 101.24(10) . . ? N1B Cu2 O13 107.46(9) . . ? O22 Cu2 C1 95.78(10) . . ? O12 Cu2 C1 30.05(10) . . ? N12B Cu2 C1 100.55(10) . . ? N1B Cu2 C1 137.59(11) . . ? O13 Cu2 C1 30.29(9) . . ? O2 Cu3 O2 83.46(9) . 2_566 ? O2 Cu3 N12C 169.26(10) . . ? O2 Cu3 N12C 96.97(10) 2_566 . ? O2 Cu3 N1C 96.50(10) . . ? O2 Cu3 N1C 164.33(10) 2_566 . ? N12C Cu3 N1C 80.19(11) . . ? O2 Cu3 O23 98.10(9) . . ? O2 Cu3 O23 102.09(9) 2_566 . ? N12C Cu3 O23 92.32(10) . . ? N1C Cu3 O23 93.45(10) . . ? O2 Cu3 Cu3 41.91(6) . 2_566 ? O2 Cu3 Cu3 41.55(6) 2_566 2_566 ? N12C Cu3 Cu3 137.52(8) . 2_566 ? N1C Cu3 Cu3 136.29(8) . 2_566 ? O23 Cu3 Cu3 103.58(7) . 2_566 ? C2A N1A C6A 119.5(3) . . ? C2A N1A Cu1 125.0(2) . . ? C6A N1A Cu1 115.5(2) . . ? N1A C2A C3A 121.8(4) . . ? C2A C3A C4A 118.9(4) . . ? C3A C4A C5A 119.7(3) . . ? C4A C5A C6A 118.6(4) . . ? N1A C6A C5A 121.6(3) . . ? N1A C6A C7A 114.5(3) . . ? C5A C6A C7A 123.9(3) . . ? N12A C7A C8A 121.8(3) . . ? N12A C7A C6A 114.6(3) . . ? C8A C7A C6A 123.6(3) . . ? C9A C8A C7A 118.1(4) . . ? C10A C9A C8A 120.1(4) . . ? C9A C10A C11A 118.9(4) . . ? N12A C11A C10A 121.4(4) . . ? C11A N12A C7A 119.7(3) . . ? C11A N12A Cu1 125.9(2) . . ? C7A N12A Cu1 114.4(2) . . ? C6B N1B C2B 118.8(3) . . ? C6B N1B Cu2 115.6(2) . . ? C2B N1B Cu2 125.6(2) . . ? N1B C2B C3B 121.9(4) . . ? C2B C3B C4B 119.3(4) . . ? C3B C4B C5B 119.4(4) . . ? C6B C5B C4B 118.1(4) . . ? N1B C6B C5B 122.4(4) . . ? N1B C6B C7B 114.1(3) . . ? C5B C6B C7B 123.5(3) . . ? N12B C7B C8B 121.4(3) . . ? N12B C7B C6B 114.2(3) . . ? C8B C7B C6B 124.4(3) . . ? C7B C8B C9B 119.2(3) . . ? C10B C9B C8B 119.2(3) . . ? C9B C10B C11B 119.1(4) . . ? N12B C11B C10B 122.3(3) . . ? C11B N12B C7B 118.9(3) . . ? C11B N12B Cu2 125.6(2) . . ? C7B N12B Cu2 115.5(2) . . ? C6C N1C C2C 118.3(3) . . ? C6C N1C Cu3 115.2(2) . . ? C2C N1C Cu3 126.5(2) . . ? N1C C2C C3C 122.2(3) . . ? C2C C3C C4C 119.7(3) . . ? C3C C4C C5C 118.8(3) . . ? C6C C5C C4C 118.8(3) . . ? N1C C6C C5C 122.2(3) . . ? N1C C6C C7C 114.1(3) . . ? C5C C6C C7C 123.7(3) . . ? N12C C7C C8C 121.6(3) . . ? N12C C7C C6C 114.6(3) . . ? C8C C7C C6C 123.8(3) . . ? C9C C8C C7C 118.9(3) . . ? C8C C9C C10C 119.1(3) . . ? C11C C10C C9C 119.3(3) . . ? N12C C11C C10C 122.3(3) . . ? C11C N12C C7C 118.8(3) . . ? C11C N12C Cu3 125.4(2) . . ? C7C N12C Cu3 115.8(2) . . ? Cu1 O1 Cu1 94.55(10) . 2_677 ? Cu3 O2 Cu3 96.54(9) . 2_566 ? O11 C1 O13 122.6(3) . . ? O11 C1 O12 121.4(3) . . ? O13 C1 O12 116.0(3) . . ? O11 C1 Cu2 170.7(2) . . ? O13 C1 Cu2 66.39(16) . . ? O12 C1 Cu2 49.70(14) . . ? C1 O12 Cu2 100.26(18) . . ? C1 O13 Cu1 117.69(19) . . ? C1 O13 Cu2 83.32(17) . . ? Cu1 O13 Cu2 138.15(11) . . ? O23 C2 O21 122.5(3) . . ? O23 C2 O22 118.1(3) . . ? O21 C2 O22 119.4(3) . . ? C2 O22 Cu2 108.3(2) . . ? C2 O23 Cu3 124.7(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.183 _refine_diff_density_min -0.988 _refine_diff_density_rms 0.105 data_2 _database_code_depnum_ccdc_archive 'CCDC 289115' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H29 Cu2 N4 O11 P' _chemical_formula_weight 659.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6485(6) _cell_length_b 34.413(2) _cell_length_c 7.7810(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.3000(10) _cell_angle_gamma 90.00 _cell_volume 2514.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Blue _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.822 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16995 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 28.48 _reflns_number_total 5718 _reflns_number_gt 4475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5718 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.82216(3) 0.164857(9) 0.38394(4) 0.01445(9) Uani 1 1 d . . . Cu2 Cu 0.92926(3) 0.089714(9) 0.30356(4) 0.01479(9) Uani 1 1 d . . . O1 O 0.98834(19) 0.13177(6) 0.4757(3) 0.0166(4) Uani 1 1 d . . . H1O H 0.976(3) 0.1250(10) 0.552(4) 0.024(10) Uiso 1 1 d . . . O2 O 0.75792(18) 0.12044(5) 0.2287(2) 0.0156(4) Uani 1 1 d . . . H2O H 0.746(3) 0.1234(9) 0.137(4) 0.025(10) Uiso 1 1 d . . . P1 P 0.71927(6) 0.118329(19) 0.71409(8) 0.01225(14) Uani 1 1 d . . . O11 O 0.69989(18) 0.14883(5) 0.5781(2) 0.0195(4) Uani 1 1 d . . . O12 O 0.68130(19) 0.13487(6) 0.8734(2) 0.0213(4) Uani 1 1 d . . . O13 O 0.62827(19) 0.08488(6) 0.6517(2) 0.0242(4) Uani 1 1 d . . . O14 O 0.87131(18) 0.10587(6) 0.7597(2) 0.0218(4) Uani 1 1 d . . . N1A N 0.9148(2) 0.21481(6) 0.4920(3) 0.0170(5) Uani 1 1 d . . . C2A C 1.0398(3) 0.21796(9) 0.6109(3) 0.0215(6) Uani 1 1 d . . . H2A H 1.082(3) 0.1951(8) 0.642(3) 0.015(7) Uiso 1 1 d . . . C3A C 1.0990(3) 0.25357(9) 0.6684(4) 0.0236(6) Uani 1 1 d . . . H3A H 1.182(3) 0.2537(9) 0.744(4) 0.026(8) Uiso 1 1 d . . . C4A C 1.0273(3) 0.28695(9) 0.6017(4) 0.0253(6) Uani 1 1 d . . . H4A H 1.059(3) 0.3097(9) 0.634(4) 0.022(8) Uiso 1 1 d . . . C5A C 0.8981(3) 0.28424(9) 0.4815(4) 0.0226(6) Uani 1 1 d . . . H5A H 0.852(3) 0.3031(8) 0.437(3) 0.008(7) Uiso 1 1 d . . . C6A C 0.8439(3) 0.24774(8) 0.4290(3) 0.0176(5) Uani 1 1 d . . . C7A C 0.7052(3) 0.24070(8) 0.3018(3) 0.0161(5) Uani 1 1 d . . . C8A C 0.6114(3) 0.27031(9) 0.2291(4) 0.0212(6) Uani 1 1 d . . . H8A H 0.632(3) 0.2951(9) 0.257(4) 0.029(8) Uiso 1 1 d . . . C9A C 0.4825(3) 0.25989(9) 0.1179(4) 0.0262(6) Uani 1 1 d . . . H9A H 0.422(3) 0.2799(10) 0.067(4) 0.035(9) Uiso 1 1 d . . . C10A C 0.4519(3) 0.22128(9) 0.0817(4) 0.0251(6) Uani 1 1 d . . . H10A H 0.366(3) 0.2128(9) 0.005(4) 0.031(8) Uiso 1 1 d . . . C11A C 0.5509(3) 0.19372(9) 0.1568(4) 0.0218(6) Uani 1 1 d . . . H11A H 0.535(3) 0.1669(9) 0.135(4) 0.021(8) Uiso 1 1 d . . . N12A N 0.6755(2) 0.20308(6) 0.2649(3) 0.0167(5) Uani 1 1 d . . . N1B N 1.0914(2) 0.05403(6) 0.4064(3) 0.0164(4) Uani 1 1 d . . . C2B C 1.2126(3) 0.06409(9) 0.5191(4) 0.0212(6) Uani 1 1 d . . . H2B H 1.214(3) 0.0886(8) 0.560(3) 0.012(7) Uiso 1 1 d . . . C3B C 1.3240(3) 0.03839(9) 0.5755(4) 0.0230(6) Uani 1 1 d . . . H3B H 1.402(3) 0.0472(9) 0.653(4) 0.032(9) Uiso 1 1 d . . . C4B C 1.3079(3) 0.00044(9) 0.5163(4) 0.0251(6) Uani 1 1 d . . . H4B H 1.377(3) -0.0197(8) 0.557(3) 0.020(7) Uiso 1 1 d . . . C5B C 1.1824(3) -0.01047(8) 0.3987(3) 0.0206(6) Uani 1 1 d . . . H5B H 1.171(3) -0.0372(9) 0.361(4) 0.027(8) Uiso 1 1 d . . . C6B C 1.0764(3) 0.01710(8) 0.3446(3) 0.0163(5) Uani 1 1 d . . . C7B C 0.9411(3) 0.00929(8) 0.2138(3) 0.0173(5) Uani 1 1 d . . . C8B C 0.9046(3) -0.02655(8) 0.1366(4) 0.0219(6) Uani 1 1 d . . . H8B H 0.969(3) -0.0444(10) 0.162(4) 0.035(9) Uiso 1 1 d . . . C9B C 0.7753(3) -0.03038(9) 0.0125(4) 0.0255(6) Uani 1 1 d . . . H9B H 0.750(3) -0.0538(9) -0.040(4) 0.029(8) Uiso 1 1 d . . . C10B C 0.6882(3) 0.00168(9) -0.0296(3) 0.0234(6) Uani 1 1 d . . . H10B H 0.599(3) 0.0007(9) -0.119(4) 0.024(7) Uiso 1 1 d . . . C11B C 0.7309(3) 0.03689(9) 0.0520(3) 0.0205(6) Uani 1 1 d . . . H11B H 0.678(3) 0.0591(8) 0.029(3) 0.013(7) Uiso 1 1 d . . . N12B N 0.8549(2) 0.04062(6) 0.1730(3) 0.0163(4) Uani 1 1 d . . . O1W O 1.0219(2) 0.11532(6) 0.0955(3) 0.0240(5) Uani 1 1 d . . . H1W1 H 0.976(4) 0.1143(11) -0.006(5) 0.053(12) Uiso 1 1 d . . . H1W2 H 1.106(4) 0.1162(10) 0.099(4) 0.033(9) Uiso 1 1 d . . . O2W O 1.3013(2) 0.12740(7) 0.1173(3) 0.0271(5) Uani 1 1 d . . . H2W1 H 1.317(3) 0.1331(9) 0.024(4) 0.026(9) Uiso 1 1 d . . . H2W2 H 1.367(4) 0.1122(10) 0.174(4) 0.036(10) Uiso 1 1 d . . . O3W O 1.3813(3) 0.14462(8) -0.1963(3) 0.0357(6) Uani 1 1 d . . . H3W1 H 1.471(4) 0.1405(10) -0.182(4) 0.040(10) Uiso 1 1 d . . . H3W2 H 1.353(4) 0.1490(10) -0.286(4) 0.030(11) Uiso 1 1 d . . . O4W O 0.5200(2) 0.08424(6) 0.2886(3) 0.0253(5) Uani 1 1 d . . . H4W1 H 0.536(3) 0.0880(9) 0.387(4) 0.021(9) Uiso 1 1 d . . . H4W2 H 0.584(4) 0.0949(11) 0.262(4) 0.041(11) Uiso 1 1 d . . . O5W O 0.2487(2) 0.16364(6) 0.4449(3) 0.0256(5) Uani 1 1 d . . . H5W1 H 0.270(4) 0.1571(11) 0.361(5) 0.044(12) Uiso 1 1 d . . . H5W2 H 0.170(4) 0.1533(10) 0.449(4) 0.035(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01348(15) 0.01261(17) 0.01640(15) -0.00048(12) 0.00167(12) 0.00073(12) Cu2 0.01375(15) 0.01305(17) 0.01653(16) -0.00054(12) 0.00133(12) 0.00138(12) O1 0.0166(9) 0.0162(11) 0.0161(9) 0.0001(8) 0.0016(8) 0.0017(7) O2 0.0162(9) 0.0167(10) 0.0125(9) -0.0006(8) 0.0005(7) 0.0006(7) P1 0.0123(3) 0.0121(3) 0.0117(3) 0.0008(2) 0.0015(2) 0.0009(2) O11 0.0198(9) 0.0196(11) 0.0204(9) 0.0031(8) 0.0072(7) 0.0049(8) O12 0.0224(9) 0.0248(11) 0.0165(9) 0.0003(8) 0.0042(7) 0.0033(8) O13 0.0235(10) 0.0219(11) 0.0260(10) -0.0019(8) 0.0030(8) -0.0030(8) O14 0.0167(9) 0.0266(11) 0.0206(9) 0.0014(8) 0.0011(7) 0.0045(8) N1A 0.0154(10) 0.0172(12) 0.0194(11) -0.0009(9) 0.0060(9) -0.0003(9) C2A 0.0205(13) 0.0240(16) 0.0199(13) -0.0014(12) 0.0046(11) 0.0008(12) C3A 0.0204(14) 0.0260(17) 0.0236(14) -0.0034(12) 0.0034(12) -0.0032(12) C4A 0.0298(15) 0.0194(16) 0.0285(15) -0.0084(13) 0.0103(12) -0.0086(13) C5A 0.0272(15) 0.0160(15) 0.0267(14) -0.0004(12) 0.0104(12) 0.0004(12) C6A 0.0202(13) 0.0164(14) 0.0191(12) -0.0002(11) 0.0104(10) 0.0003(10) C7A 0.0181(12) 0.0148(14) 0.0171(12) 0.0003(10) 0.0076(10) 0.0006(10) C8A 0.0247(14) 0.0143(15) 0.0258(14) 0.0014(12) 0.0082(11) -0.0003(11) C9A 0.0278(15) 0.0246(17) 0.0259(14) 0.0058(13) 0.0056(12) 0.0105(13) C10A 0.0197(14) 0.0228(16) 0.0304(15) -0.0017(13) 0.0012(12) 0.0026(12) C11A 0.0186(13) 0.0200(16) 0.0259(14) -0.0009(12) 0.0031(11) -0.0003(11) N12A 0.0155(10) 0.0150(12) 0.0197(11) 0.0012(9) 0.0046(8) 0.0007(9) N1B 0.0159(10) 0.0142(12) 0.0184(10) 0.0023(9) 0.0026(8) 0.0020(9) C2B 0.0202(13) 0.0185(16) 0.0234(13) 0.0019(12) 0.0021(11) -0.0007(11) C3B 0.0174(13) 0.0259(17) 0.0247(14) 0.0075(12) 0.0024(11) -0.0010(12) C4B 0.0193(13) 0.0267(17) 0.0306(15) 0.0079(13) 0.0088(12) 0.0087(12) C5B 0.0228(13) 0.0156(15) 0.0255(14) 0.0027(12) 0.0101(11) 0.0024(11) C6B 0.0184(12) 0.0155(14) 0.0166(12) 0.0033(10) 0.0076(10) 0.0000(10) C7B 0.0199(13) 0.0153(14) 0.0188(12) 0.0003(11) 0.0086(10) 0.0010(10) C8B 0.0244(14) 0.0166(15) 0.0256(14) 0.0015(12) 0.0074(12) 0.0018(12) C9B 0.0308(16) 0.0198(16) 0.0261(15) -0.0072(12) 0.0072(12) -0.0067(13) C10B 0.0223(14) 0.0275(17) 0.0199(13) -0.0032(12) 0.0038(11) -0.0038(12) C11B 0.0200(13) 0.0198(16) 0.0207(13) -0.0004(11) 0.0027(11) 0.0018(11) N12B 0.0168(11) 0.0139(12) 0.0177(10) 0.0002(9) 0.0031(8) 0.0002(9) O1W 0.0151(10) 0.0357(13) 0.0208(11) 0.0010(9) 0.0032(9) -0.0040(9) O2W 0.0182(10) 0.0321(13) 0.0312(12) 0.0008(10) 0.0060(9) -0.0039(9) O3W 0.0199(12) 0.0606(18) 0.0262(13) 0.0009(12) 0.0045(10) 0.0035(11) O4W 0.0221(11) 0.0310(13) 0.0219(11) -0.0012(9) 0.0034(9) -0.0064(9) O5W 0.0215(11) 0.0271(12) 0.0275(11) -0.0038(9) 0.0036(9) -0.0034(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.9581(18) . ? Cu1 O1 1.9623(18) . ? Cu1 N12A 1.997(2) . ? Cu1 N1A 2.029(2) . ? Cu1 O11 2.1907(17) . ? Cu1 Cu2 2.9057(5) . ? Cu2 O2 1.9358(18) . ? Cu2 O1 1.9652(19) . ? Cu2 N1B 2.005(2) . ? Cu2 N12B 2.016(2) . ? Cu2 O1W 2.2047(19) . ? P1 O13 1.461(2) . ? P1 O11 1.4714(18) . ? P1 O12 1.4847(18) . ? P1 O14 1.4906(18) . ? N1A C2A 1.345(3) . ? N1A C6A 1.356(3) . ? C2A C3A 1.382(4) . ? C3A C4A 1.379(4) . ? C4A C5A 1.379(4) . ? C5A C6A 1.386(4) . ? C6A C7A 1.490(4) . ? C7A N12A 1.342(3) . ? C7A C8A 1.393(4) . ? C8A C9A 1.389(4) . ? C9A C10A 1.376(4) . ? C10A C11A 1.377(4) . ? C11A N12A 1.339(3) . ? N1B C2B 1.336(3) . ? N1B C6B 1.355(3) . ? C2B C3B 1.383(4) . ? C3B C4B 1.382(4) . ? C4B C5B 1.391(4) . ? C5B C6B 1.387(4) . ? C6B C7B 1.483(3) . ? C7B N12B 1.354(3) . ? C7B C8B 1.381(4) . ? C8B C9B 1.397(4) . ? C9B C10B 1.380(4) . ? C10B C11B 1.386(4) . ? C11B N12B 1.348(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O1 83.55(8) . . ? O2 Cu1 N12A 97.94(8) . . ? O1 Cu1 N12A 169.60(9) . . ? O2 Cu1 N1A 164.55(8) . . ? O1 Cu1 N1A 95.50(8) . . ? N12A Cu1 N1A 80.30(8) . . ? O2 Cu1 O11 94.85(7) . . ? O1 Cu1 O11 97.33(8) . . ? N12A Cu1 O11 92.81(7) . . ? N1A Cu1 O11 100.56(7) . . ? O2 Cu1 Cu2 41.44(5) . . ? O1 Cu1 Cu2 42.32(5) . . ? N12A Cu1 Cu2 137.36(6) . . ? N1A Cu1 Cu2 134.33(6) . . ? O11 Cu1 Cu2 101.48(5) . . ? O2 Cu2 O1 84.06(8) . . ? O2 Cu2 N1B 171.34(8) . . ? O1 Cu2 N1B 95.84(8) . . ? O2 Cu2 N12B 97.24(8) . . ? O1 Cu2 N12B 166.96(8) . . ? N1B Cu2 N12B 80.93(8) . . ? O2 Cu2 O1W 91.33(8) . . ? O1 Cu2 O1W 95.91(8) . . ? N1B Cu2 O1W 97.28(8) . . ? N12B Cu2 O1W 97.03(8) . . ? O2 Cu2 Cu1 42.03(5) . . ? O1 Cu2 Cu1 42.24(5) . . ? N1B Cu2 Cu1 137.96(6) . . ? N12B Cu2 Cu1 138.69(6) . . ? O1W Cu2 Cu1 91.52(6) . . ? Cu1 O1 Cu2 95.44(8) . . ? Cu2 O2 Cu1 96.53(8) . . ? O13 P1 O11 110.83(11) . . ? O13 P1 O12 109.55(11) . . ? O11 P1 O12 108.18(11) . . ? O13 P1 O14 109.62(11) . . ? O11 P1 O14 109.37(10) . . ? O12 P1 O14 109.26(10) . . ? P1 O11 Cu1 132.53(11) . . ? C2A N1A C6A 118.6(2) . . ? C2A N1A Cu1 126.39(19) . . ? C6A N1A Cu1 114.89(17) . . ? N1A C2A C3A 122.2(3) . . ? C4A C3A C2A 118.9(3) . . ? C3A C4A C5A 119.7(3) . . ? C4A C5A C6A 118.9(3) . . ? N1A C6A C5A 121.7(2) . . ? N1A C6A C7A 113.9(2) . . ? C5A C6A C7A 124.3(2) . . ? N12A C7A C8A 122.1(2) . . ? N12A C7A C6A 114.4(2) . . ? C8A C7A C6A 123.4(2) . . ? C9A C8A C7A 118.0(3) . . ? C10A C9A C8A 119.7(3) . . ? C9A C10A C11A 118.9(3) . . ? N12A C11A C10A 122.4(3) . . ? C11A N12A C7A 118.9(2) . . ? C11A N12A Cu1 124.83(19) . . ? C7A N12A Cu1 116.28(17) . . ? C2B N1B C6B 118.8(2) . . ? C2B N1B Cu2 126.01(19) . . ? C6B N1B Cu2 115.04(16) . . ? N1B C2B C3B 122.8(3) . . ? C4B C3B C2B 118.6(3) . . ? C3B C4B C5B 119.2(3) . . ? C6B C5B C4B 119.0(3) . . ? N1B C6B C5B 121.5(2) . . ? N1B C6B C7B 114.7(2) . . ? C5B C6B C7B 123.7(2) . . ? N12B C7B C8B 121.8(2) . . ? N12B C7B C6B 114.4(2) . . ? C8B C7B C6B 123.8(2) . . ? C7B C8B C9B 118.8(3) . . ? C10B C9B C8B 119.1(3) . . ? C9B C10B C11B 119.3(3) . . ? N12B C11B C10B 121.8(3) . . ? C11B N12B C7B 119.1(2) . . ? C11B N12B Cu2 125.99(19) . . ? C7B N12B Cu2 114.88(16) . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 28.48 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 0.542 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.104